CN106674830B - 一种多孔非金属材料 - Google Patents

一种多孔非金属材料 Download PDF

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CN106674830B
CN106674830B CN201510767126.6A CN201510767126A CN106674830B CN 106674830 B CN106674830 B CN 106674830B CN 201510767126 A CN201510767126 A CN 201510767126A CN 106674830 B CN106674830 B CN 106674830B
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polytetrafluoroethylene
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CN106674830A (zh
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叶雷
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Chongqing Runze Pharmaceutical Co Ltd
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Chongqing Runze Pharmaceutical Co Ltd
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Priority to US16/075,993 priority patent/US20200239658A1/en
Priority to PCT/CN2016/104836 priority patent/WO2017080415A1/zh
Priority to EP16863591.0A priority patent/EP3409720A4/en
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Abstract

本发明提供了一种多孔非金属材料，包括材料本体，本体具有孔腔，及呈三维空间围绕孔腔形成的腔壁构成，其孔腔呈均匀性分布，各孔腔均三维贯通，孔腔呈均匀性分布是指各孔腔在多孔材料上任意单位级体积下呈均匀性分布。本发明对多孔材料的孔腔分布均匀提出了具体而明确的度量方式，明确了是以小单位级体积的尺度下来度量多孔材料以及其多级结构的孔分布均匀性，这样的多孔结构是高度均匀的，从而保证了多孔材料的各个性能的均匀一致性。

Description

一种多孔非金属材料
技术领域
本发明涉及一种多孔材料，特别是一种多孔非金属材料。
背景技术
含一定数量孔洞的固体叫多孔材料，是一种由贯通或封闭的孔洞构成网络结构的材料。相对连续介质材料而言，多孔材料一般具有相对密度低、比强度高、比表面积高、重量轻、隔音、隔热、渗透性好等优点。按照孔径大小的不同，多孔材料又可以分为微孔(孔径小于2nm)材料、介孔(孔径2-50nm)材料和大孔(孔径大于50nm)材料。
多孔材料按其材质区分，可分为金属多孔材料和非金属多孔材料。非金属多孔材料一般具有比表面积大、密度小、热导率小、相对密度小、孔隙率大等特点，在催化剂(包括载体)、吸附剂、保温、绝热、污水和废气处理、过滤液体和气体(甚至细菌)、轻质建筑材料，环保、改良土壤、化工等领域具有广泛的应用前景。
CN104355302公开了一种轻质纳米多孔材料碳气凝胶的制备方法，其以氧化石墨烯交联聚酰胺酸气凝胶制备而成，内部具有50-200nm，1.4nm和13-40nm的不同孔洞。由于孔结构的随机性、不规则性，制备方法不能制备出规则的孔，这种结构的多孔材料仍然不能满足应用性能。
在很多应用中，都需要其多孔材料本身均匀，其孔径大小、孔的分布均匀，使得性能均匀一致，但实际上，很多多孔材料达不到此要求，其均匀性补足；尽管有的材料自称达到了较高的均匀性，但其均匀性仍是大体积尺度下的均匀性，若用小体积尺度进行衡量，比如在材料上任取多块体积不大于一立方厘米的三维体，分别测其质量，其均匀程度差异仍然非常大，因此造成多孔材料的各种性能如强度、弹性模量等的不均匀，严重影响其功能。
发明内容
本发明的目的在于给出结构适宜、可控、高度均匀的多孔非金属材料。
本发明的目的是通过以下措施实现的：
一种多孔非金属材料，包括材料本体，本体具有孔腔，及呈三维空间围绕孔腔形成的腔壁构成，其孔腔呈均匀性分布，各孔腔均三维贯通，孔腔呈均匀性分布是指各孔腔在多孔材料上任意单位级体积下呈均匀性分布。
具体地，上述单位级体积是指立方厘米级或立方毫米级或更小单位级体积。
更具体地，上述孔腔呈均匀性分布是指在该多孔材料上任取的体积不大于一立方厘米且相同大小的各三维体，它们的质量基本相当。
更具体地，上述质量基本相当是指在多孔材料上任取的多个体积不大于一立方厘米且相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。
进一步地，在该多级材料上任取的体积不大于一立方毫米的相同大小的三维体，它们质量基本相当。
更具体地，所述质量基本相当是指在多孔材料上任取的多个体积不大于一立方毫米的相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4％。
优选地，上述多孔非金属材料由多级多孔材料构成，本体是以材料孔径大小进行分级的孔腔，及呈三维空间围绕孔腔的腔壁构成，腔壁上设置下级孔腔，各级孔腔均各自三维贯通且各级孔腔相互间也彼此贯通。更具体地，下一级多孔材料构成上一级孔腔的腔壁。上级孔腔的腔壁是由其下级的多级多孔材料复合构成，或是由其下级的各级多孔材料复合构成，可使得材料满足特定的功能需求。
具体地，材料本体的每级多孔材料自为一连续结构体。每一级多孔材料的最大外边界与整个材料本体空间边界相当。即每级多孔材料可以作为一级独立的多孔材料存在于本体中，且具有其独自的物化性能。这样的结构可以使得各级多孔材料的物化性能有所差异，在相对固定的材料整个空间中具有不同的物化性能，更好的满足多方面的功能需求。
上述多孔非金属材料可以为陶瓷材料、碳素材料、玻璃材料、纤维材料、胶凝材料等。
例如，一种多孔非金属材料，包括聚四氟乙烯材料本体，其具有100nm～500μm孔径的孔腔以及呈三维空间围绕孔腔形成的腔壁，其孔腔呈均匀性分布，各孔腔均三维贯通，孔腔呈均匀性分布是指各孔腔在多孔材料上任意单位级体积下呈均匀性分布。
上述多孔非金属材料，由多级多孔聚四氟乙烯材料构成，本体是以材料孔径大小进行分级的孔腔，及呈三维空间围绕孔腔的腔壁构成，腔壁上设置10～100nm的下级孔腔，各级孔腔均各自三维贯通且各级孔腔相互间也彼此贯通。更具体地，上级孔腔的腔壁是由其下级的多级多孔材料复合构成，或是由其下级的各级多孔材料复合构成，可使得材料满足特定的功能需求。
有益效果
1.本发明提供了一种具有多孔结构的材料，明确了其结构形式，其孔腔的分级结构形式及其均匀性结构使其能满足多种功能需求。
2.本发明对多孔材料的孔腔分布均匀提出了具体而明确的度量方式，明确了是以小单位级体积的尺度下来度量多孔材料以及其多级结构的孔分布均匀性，这样的多孔结构是高度均匀的，从而保证了多孔材料的各个性能的均匀一致性。
3.本发明的多孔材料是三维贯通的，包括每级孔三维连通，以及各级孔相互三维贯通，贯通性好，能充分满足材料的功能需求。
具体实施方式
具体实施方式以本发明技术方案为前提，给出了详细的实施方式，但本发明的保护范围不仅限于下述实施方式。在不脱离和改变本发明上述技术思想情况下，根据本领域的普通技术知识和/或惯用手段，显然还可以做出多种形式的替换或变更，并均应包括在本发明的范围之内。
实施例1
本发明的多孔材料为聚四氟乙烯，具有二级孔结构，其中，均匀分布、相互贯通的第一级孔腔的腔壁上有均匀分布、相互贯通的第二级孔腔，且两级孔相互之间也彼此贯通，所述贯通为三维贯通。材料本体的每级多孔材料自为一连续结构体。总有效孔隙率为70％，大孔平均孔径为0.45μm，在大孔的腔壁上有平均孔径30nm的贯通小孔。
用机械加工方法在该多孔材料上任取9件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，结果如表1所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表1可知，其质量偏差不大于4％。
表1
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 655.815 0.6％
2 633.422 2.9％
3 645.542 1.0％
4 665.844 2.1％
5 640.038 1.9％
6 675.967 3.6％
7 643.786 1.3％
8 658.871 1.0％
9 650.425 0.3％
质量平均值 652.19
该聚四氟乙烯多孔材料的制备方法是：
(1)将固含量60％的聚四氟乙烯乳液，粒径30nm壳聚糖、5％(质量比)海藻酸钠溶液，均匀混合，按照50∶30∶4质量比，配成纺丝液；
(2)在真空条件下，在取向静电纺纤维丝装置中采用静电纺丝方法制取聚四氟乙烯前驱膜；
(3)将前驱膜缠绕5层到圆筒支撑模上，送入管式炉中在真空或保护气氛中烧结，烧结采用程序控温分段连续烧结，以5℃/min的速率从室温升温到150℃，在150℃保温60min；以5℃/min的速率升温到400℃，在400℃保温120min。
(4)烧结后程序控温冷却，按照常规技术后续处理，得到具有两级孔结构的多孔聚四氟乙烯中空纤维膜。
该材料可用于气液分离和液液分离，实现精确分级过滤，比如其适用于两元或多元气(液)体(如挥发性溶质水溶液)的滤过，同时其通量大，截留率、分离系数高，疏水性能优，不易被污染(如液体浸润)，具有高效长效的优势。
实施例2
本发明的多孔材料为多孔陶瓷，具有三级孔结构，其中，均匀分布、相互贯通的第一级孔腔的腔壁上有均匀分布、相互贯通的第二级孔腔，第二级孔腔的孔壁上有均匀分布、相互贯通的第三季孔腔，且三级孔相互之间也彼此贯通，所述贯通为三维贯通。材料本体的每级多孔材料自为一连续结构体。每一级多孔材料的最大外边界与整个材料本体空间边界相当。总有效孔隙率为75％，大孔平均孔径为500μm，在大孔的腔壁上有平均孔径30μm的贯通二级孔，在第二级孔的孔壁上有平均孔径800nm贯通的第三级孔。
用机械加工方法在该多孔材料上任取9件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，结果如表2所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表2可知，其质量偏差不大于4％。
表2
件号 质量(mg) 相对于平均值的偏差绝对值(％)
1 1254.855 2.4％
2 1300.448 1.2％
3 1280.488 0.4％
4 1310.841 2.0％
5 1265.184 1.6％
6 1279.941 0.4％
7 1293.218 0.6％
8 1280.215 0.4％
9 1305.565 1.5％
质量平均值 1285.639
该多孔陶瓷的制备方法是：
(1)选取粒径为800±50nm的聚苯乙烯小球，将其组装形成三维有序排列的胶体模板，制备陶瓷纳米溶液，将钽纳米溶液引入聚苯乙烯小球制成的三维胶体模板中，将三维胶体模板/陶瓷纳米溶液的混合物干燥，然后破碎为粒径为5μm的颗粒；
(2)取粒径为800±50nm的淀粉，按照重量比例1∶50与蒸馏水混合，制成淀粉溶液，将上述颗粒、粒径为30μm的乙基纤维素及淀粉溶液按照重量比15∶2∶7制成浆料，均匀浸渍到孔径为550±20μm的聚氨酯泡沫上；
(3)将浸渍后的聚氨酯泡沫在真空或保护气氛中烧结，再按照多孔陶瓷制备工艺进行常规处理，制得具有三级孔的多孔陶瓷。
该种多级陶瓷可以作为医用植入材料，第一级孔尺寸特别适用于满足血管等生命组织长入的需求；第二级孔特有适于多孔细胞的寄居，第三级孔因其大量的纳米孔特别有利于满足细胞的粘附、分化需求，且比表面积大，能负载很多生长因子，而且，孔的贯通性好，各级孔均各自相互贯通且各级孔相互之间也彼此贯通，能充分满足血液、组织液的浸润、传输，实现蛋白质降解产物及新陈代谢产物的排出，因此它是一种真正的骨再生材料。
实施例3
本发明的多孔材料为多孔玻璃，具有二级孔结构，其中，均匀分布、相互贯通的第一级孔腔的腔壁上有均匀分布、相互贯通的第二级孔腔，第二级孔腔的孔壁上有均匀分布、相互贯通的第三季孔腔，且三级孔相互之间也彼此贯通，所述贯通为三维贯通。材料本体的每级多孔材料自为一连续结构体。每一级多孔材料的最大外边界与整个材料本体空间边界相当。总有效孔隙率为80％，大孔平均孔径为20μm，在大孔的腔壁上有平均孔径800nm的贯通二级孔，在第二级孔的孔壁上有平均孔径10nm贯通的第三级孔。
用机械加工方法在该多孔材料上任取9件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，结果如表3所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表3可知，其质量偏差不大于4％。
表3
Figure GDA0000908878410000051
Figure GDA0000908878410000061
制备方法：
(1)以纯的SiO2、H3BO3、Na2CO3为主要原料，按照Na2O10％、B2O325％、SiO265％(摩尔百分比)配料，在1400℃熔融，不断搅拌保温4小时，然后浇铸模具成型；
(2)分相：采用程序控温，以25℃/min的速率从室温升温到520℃保温24小时；以20℃/min的速率升温到670℃，在670℃保温36小时；然后以5-10℃/min降温冷却；
(3)在95℃在1-2mol/L酸液浸析，经清洗、干燥、破碎等后处理得到纳米玻璃微珠；
(4)将粒径为20μm甲基纤维素、微珠按照3∶1体积比均匀混合后均匀灌入三维贯通的聚酯泡沫，然后经压制为致密胚体；
(5)将真空烧结、退火、冷却等常规热处理得到三级孔的多孔玻璃。
该种多级玻璃可以作为多种用途的载体，如物质的反应模板，制成多级的纳米微米级产物；如催化剂载体或药物缓释载体，具有用量少，效率高，恒定、均匀、长效的优势。
实施例4
本发明的多孔材料为聚四氟乙烯，具有三级孔结构，其中，均匀分布、相互贯通的第一级孔腔的腔壁上有均匀分布、相互贯通的第二级孔腔，且两级孔相互之间也彼此贯通，所述贯通为三维贯通。材料本体的每级多孔材料自为一连续结构体。总有效孔隙率为80％，大孔平均孔径为1000nm，在大孔的腔壁上有平均孔径100nm的贯通二级孔，在第二级孔的孔壁上有平均孔径10nm贯通的第三级孔。
用机械加工方法在该多孔材料上任取9件10mm×10mm×10mm的相同尺寸的三维体，用梅特勒-托利多XP26Microbalance天平测试其质量，结果如表1所示，其中，相对于平均值的偏差绝对值用百分比表示，其值为相对于平均值的偏差绝对值除以质量平均值，由表4可知，其质量偏差不大于4％。
表4
Figure GDA0000908878410000062
Figure GDA0000908878410000071
该聚四氟乙烯多孔材料的制备方法是：
(1)将PTFE细粉末、分子量为1000的聚乙二醇混合，搅拌加热至380℃，持续搅拌60min，快速冷却至室温进行破碎，在零下摄氏度进行粉碎得到聚四氟乙烯颗粒；
(2)将粒径为200nm聚四氟乙烯颗粒分散配置为固含量60％乳液，将其与粒径100nm壳聚糖、5％(质量比)海藻酸钠溶液，均匀混合，按照50∶30∶4质量比，配成纺丝液；
(3)在真空条件下，在取向静电纺纤维丝装置中采用静电纺丝方法制取聚四氟乙烯前驱膜；
(4)将前驱膜缠绕5层到圆筒支撑模上，送入管式炉中在真空或保护气氛中烧结，烧结采用程序控温分段连续烧结，以6℃/min的速率从室温升温到160℃，在160℃保温100min；以6℃/min的速率升温到280℃，保温60min；以6℃/min的速率升温到400℃，在400℃保温100min。
(5)烧结后程序控温冷却，按照常规技术后续处理，得到具有三级孔结构的多孔聚四氟乙烯中空膜。
该材料可用于气液分离和液液分离，实现精确分级过滤，比如其适用于两元或多元气(液)体(如挥发性溶质水溶液)的滤过，同时其通量大，截留率、分离系数高，疏水性能优，不易被污染(如液体浸润)，具有高效长效的优势。

Claims (6)

1.一种多孔非金属材料，包括材料本体，本体具有孔腔，本体是以材料孔径大小进行分级的孔腔，及呈三维空间围绕孔腔的腔壁构成，腔壁上设置下级孔腔，各级孔腔均各自三维贯通且各级孔腔相互间也彼此贯通；其孔腔呈均匀性分布，孔腔呈均匀性分布是指各孔腔在多孔材料上任意单位级体积下呈均匀性分布；所述单位级体积是指立方厘米级或立方毫米级；均匀性分布是指单位级体积下任一三维体相对于质量平均值的偏差绝对值不大于三维体质量平均值的4%；
所述材料为聚四氟乙烯材料，所述聚四氟乙烯多孔材料的制备方法为：
（1）将固含量60% 的聚四氟乙烯乳液，粒径30nm 壳聚糖、5wt%海藻酸钠溶液，均匀混合，按照50：30：4质量比，配成纺丝液；
（2）在真空条件下，在取向静电纺纤维丝装置中采用静电纺丝方法制取聚四氟乙烯前驱膜；
（3）将前驱膜缠绕5 层到圆筒支撑模上，送入管式炉中在真空或保护气氛中烧结，烧结采用程序控温分段连续烧结，以5℃/min 的速率从室温升温到150℃，在150℃保温60min；以5℃/min的速率升温到400℃，在400℃保温120min；
（4）烧结后程序控温冷却，按照常规技术后续处理，得到具有两级孔结构的多孔聚四氟乙烯中空纤维膜；
或者，所述聚四氟乙烯多孔材料的制备方法为：
（1）将PTFE 细粉末、分子量为1000的聚乙二醇混合，搅拌加热至380℃，持续搅拌60min，快速冷却至室温进行破碎，在零下摄氏度进行粉碎得到聚四氟乙烯颗粒；
（2）将粒径为200nm 聚四氟乙烯颗粒分散配置为固含量60% 乳液，将其与粒径100nm壳聚糖、5wt%海藻酸钠溶液，均匀混合，按照50：30：4质量比，配成纺丝液；
（3）在真空条件下，在取向静电纺纤维丝装置中采用静电纺丝方法制取聚四氟乙烯前驱膜；
（4）将前驱膜缠绕5 层到圆筒支撑模上，送入管式炉中在真空或保护气氛中烧结，烧结采用程序控温分段连续烧结，以6℃/min 的速率从室温升温到160℃，在160℃保温100min；以6℃/min 的速率升温到280℃，保温60min ；以6℃/min 的速率升温到400℃，在400℃保温100min；
（5）烧结后程序控温冷却，按照常规技术后续处理，得到具有三级孔结构的多孔聚四氟乙烯中空膜；
或者，所述材料为多孔陶瓷材料，所述多孔陶瓷的制备方法为：
（1）选取粒径为800±50nm的聚苯乙烯小球，将其组装形成三维有序排列的胶体模板，制备陶瓷纳米溶液，将钽纳米溶液引入聚苯乙烯小球制成的三维胶体模板中，将三维胶体模板/ 陶瓷纳米溶液的混合物干燥，然后破碎为粒径为5μm 的颗粒；
（2）取粒径为800±50nm的淀粉，按照重量比例1:50 与蒸馏水混合，制成淀粉溶液，将上述颗粒、粒径为30μm的乙基纤维素及淀粉溶液按照重量比15:2:7 制成浆料，均匀浸渍到孔径为550±20μm的聚氨酯泡沫上；
（3）将浸渍后的聚氨酯泡沫在真空或保护气氛中烧结，再按照多孔陶瓷制备工艺进行常规处理，制得具有三级孔的多孔陶瓷；
或者，所述材料为多孔玻璃材料，所述多孔玻璃材料的制备方法为：
(1) 以纯的SiO2、H3BO3、Na2CO3为主要原料，按照Na2O10％、B2O325％、SiO265mol％配料，在1400℃熔融，不断搅拌保温4 小时，然后浇铸模具成型；
(2) 分相：采用程序控温，以25℃/min 的速率从室温升温到520℃保温24 小时；以20℃/min 的速率升温到670℃，在670℃保温36小时；然后以5-10℃/min 降温冷却；
(3) 在95℃在1-2mol/L 酸液浸析，经清洗、干燥、破碎后处理得到纳米玻璃微珠；
(4) 将粒径为20μm甲基纤维素、微珠按照3∶1 体积比均匀混合后均匀灌入三维贯通的聚酯泡沫，然后经压制为致密胚体；
(5) 真空烧结、退火、冷却、常规热处理得到三级孔的多孔玻璃。
2.如权利要求1所述的多孔非金属材料，所孔腔呈均匀性分布是指在该多孔材料上任取的体积不大于一立方厘米且相同大小的各三维体，它们的质量基本相当；所述质量基本相当是指在多孔材料上任取的多个体积不大于一立方厘米且相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4%。
3.如权利要求1所述的多孔非金属材料，在该多级材料上任取的体积不大于一立方毫米的相同大小的三维体，它们质量基本相当；所述质量基本相当是指在多孔材料上任取的多个体积不大于一立方毫米的相同大小的三维体，分别称其质量，得到它们质量的平均值，而任一三维体质量相对于质量平均值的偏差绝对值不大于三维体质量平均值的4%。
4.如权利要求1、2或3所述的多孔非金属材料，下一级多孔材料构成上一级孔腔的腔壁。
5.如权利要求1、2或3所述的多孔非金属材料，上级孔腔的腔壁是由其下级的多级多孔材料复合构成。
6.如权利要求4所述的多孔非金属材料，上级孔腔的腔壁是由其下级的多级多孔材料复合构成。
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